食品安全质量检测学报
食品安全質量檢測學報
식품안전질량검측학보
FOOD SAFETY AND QUALITY DETECTION TECHNOLOGY
2013年
6期
1841-1846
,共6页
魏欣欣%窦彩云%段永生%马育松
魏訢訢%竇綵雲%段永生%馬育鬆
위흔흔%두채운%단영생%마육송
阿维菌素%高压液相色谱法%辣椒干%农药残留
阿維菌素%高壓液相色譜法%辣椒榦%農藥殘留
아유균소%고압액상색보법%랄초간%농약잔류
avermectin%HPLC-FLD%dried chili%pesticide residues
目的:建立辣椒干中阿维菌素残留量的高压液相色谱-荧光检测器分析方法。方法样品采用乙腈提取,乙腈饱和的正己烷去脂,石墨化碳固相萃取小柱净化,以三氟乙酸酐(trifluoroacetic anhtdride, TFAA)和N-甲基咪唑(1-methylimidazole, NMIM)的乙腈溶液衍生化,用 C18柱分离,在激发波长为365 nm,发射波长470 nm的条件下高压液相色谱-荧光法检测。结果方法在10~500 ng/mL的浓度范围内线性关系良好,相关系数为r=0.999,检测限为5μg/kg。3个不同浓度水平上进行了加标回收率在90.3%~103.1%, RSD在2.31%~6.93%。结论该方法简便灵敏,准确快速,可用于辣椒干中阿维菌素残留量的测定。
目的:建立辣椒榦中阿維菌素殘留量的高壓液相色譜-熒光檢測器分析方法。方法樣品採用乙腈提取,乙腈飽和的正己烷去脂,石墨化碳固相萃取小柱淨化,以三氟乙痠酐(trifluoroacetic anhtdride, TFAA)和N-甲基咪唑(1-methylimidazole, NMIM)的乙腈溶液衍生化,用 C18柱分離,在激髮波長為365 nm,髮射波長470 nm的條件下高壓液相色譜-熒光法檢測。結果方法在10~500 ng/mL的濃度範圍內線性關繫良好,相關繫數為r=0.999,檢測限為5μg/kg。3箇不同濃度水平上進行瞭加標迴收率在90.3%~103.1%, RSD在2.31%~6.93%。結論該方法簡便靈敏,準確快速,可用于辣椒榦中阿維菌素殘留量的測定。
목적:건립랄초간중아유균소잔류량적고압액상색보-형광검측기분석방법。방법양품채용을정제취,을정포화적정기완거지,석묵화탄고상췌취소주정화,이삼불을산항(trifluoroacetic anhtdride, TFAA)화N-갑기미서(1-methylimidazole, NMIM)적을정용액연생화,용 C18주분리,재격발파장위365 nm,발사파장470 nm적조건하고압액상색보-형광법검측。결과방법재10~500 ng/mL적농도범위내선성관계량호,상관계수위r=0.999,검측한위5μg/kg。3개불동농도수평상진행료가표회수솔재90.3%~103.1%, RSD재2.31%~6.93%。결론해방법간편령민,준학쾌속,가용우랄초간중아유균소잔류량적측정。
Objective To establish an HPLC with fluorescence dedection method for determination of avermectin residues in dried chili. Methods Residues are extracted with acetonitrile. The extract was cleaned up with acetonitrile saturated n-hexane and graphitized carbon solid-phase extraction cartridge. Avermectin re-sidues were derived with trifluoroacetic acid and 1-methylimidazole and determined by reversed-phase liquid chromatography with fluorescence detection (excitation:365 nm and emission:470 nm). Results Recoveries ranged from 90.3% to 103.1% with RSD of 2.31~6.93% at spiking levels of 5, 10, 20 μg/kg. This method showed a good linearity over the range of 10~500 ng/mL with r=0.999. Conclusion This method is accurate, rapid, and highly sensitive and it is suitable for determination of avermectin residues in dried chili.